Current Issue : April - June Volume : 2016 Issue Number : 2 Articles : 14 Articles
The main objective of the study was to develop and validate simple, sensitive, precise and cost effective method for the estimation of canagliflozin in bulk and pharmaceutical dosage form as per ICH guidelines. Two simple spectrophotometric methods have been developed for determination of canagliflozin from tablet dosage form. First method was area under curve method where area under curve in the range of 275.2 - 304.8 nm was selected for the analysis. Second method was first order derivative spectrophotometric method in which absorbance was measured at λmin= 273.2 nm, λmax = 311.6 nm and Zero cross = 289.84 nm. Linearity for detector response was observed in the concentration range of 10-35 µg/ml at the λmax= 290.6 nm. The accuracy and precision of the methods were determined and validated statically. Both the methods showed good reproducibility and recovery with % RSD less than 2. The proposed methods were found to be rapid, reliable, specific, precise and accurate and hence can be successfully applied for the routine analysis of canagliflozin in bulk and pharmaceutical dosage forms....
Aim of this research was to develop a simple, precise, accurate and reproducible absorbance ratio method for estimation of amiodaroone HCl and ranolazine in combination of synthetic mixture in 1: 10 ratios and validate it as per ICH guidelines. Methanol selected as a solvent for estimation of amiodarone HCl at 258.62 nm and for ranolazine at 273.00 nm in linearity range 1-20 µg/ml and 10-200 µg/ml respectively. The correlation coefficient (r2) for amiodarone HCl was 0.9998 and for ranolazine 0.9996. The mean % recovery was found to be in range of 99.77%-101.22% for amiodarone HCl and 99.90%-100.58% for ranolazine. The result of analysis has been validated statistically and recovery studies recommended for routine since it is rapid, simple, accurate, sensitive....
A simple, accurate and precise spectroscopic method was developed for simultaneous estimation of aripiprazole and escitalopram oxalate in synthetic mixture using simultaneous equation method. In this spectroscopic method, 255.00 nm and 238.00 nm wavelengths were selected for measurement of absorptivity. Both the drugs show linearity in a concentration range of 5-30 μg/ml and 15-75 μg/ml at their respective λmax. Accuracy, precision and recovery studies were done by QC samples covering lower, medium and high concentrations of the linearity range. The relative standard deviation for accuracy, precision studies were found to be within the acceptance range (<2%). The limit of determination was 0.129 and 0.223 μg/ml aripiprazole and escitalopram oxalate, respectively. The limit of quantification was 0.392 and 0.677 for aripiprazole and escitalopram oxalate, respectively. Recovery of aripiprazole and escitalopram oxalate was found to be 100.66 % and 100.70 % respectively confirming the accuracy of the proposed method. The proposed method is recommended for routine analysis since it is rapid, simple, accurate, sensitive and specific by no heating and no organic solvent extraction....
Aim of this research was to develop a simple, precise, accurate and reproducible first order derivative method spectrophotometric method for estimation of aripiprazole and escitalopram oxalate in combination of synthetic mixture in 1: 3 ratios and validate it as per ICH guidelines. The method is based on first order UV derivative spectrophotometry. Methanol was selected as a solvent for estimation of aripiprazole at ZCP of escitalopram oxalate 297 nm and for escitalopram oxalate at ZCP of aripiprazole 286 nm in linearity range 5-25 µg/ml and 15-75 µg/ml respectively. The correlation coefficient (r2) for aripiprazole was 0.995 and for escitalopram oxalate 0.997. The mean % recovery was found to be in range of 99.55%-101.00% for aripiprazole and 100.15%-101.16% for escitalopram oxalate. The result of analysis has been validated statistically and recovery studies recommended for routine since it is rapid, simple, accurate and sensitive....
Aim of this research was to develop a simple, precise, accurate and reproducible first order derivative method spectrophotometry method for estimation of ivabradine HCl and atenolol in combination of synthetic mixture in 1:10 ratios and validate it as per ICH guidelines. The method is based on first order UV derivative spectrophotometry. Methanol was selected as a solvent for estimation of ivabradine HCl at ZCP of atenolol 299.30 nm and for atenolol at ZCP of ivabradine HCl 287.00 nm in linearity range 2-10 µg/ml and 20-100 µg/ml respectively. The correlation coefficient (r2) for ivabradine HCl was 0.9999 and for atenolol 0.9994. The mean % recovery was found to be in range of 100.23%-101.00% for ivabradine HCl and 100.17%-101.41% for atenolol. The result of analysis has been validated statistically and recovery studies recommended for routine since it is rapid, simple, accurate, sensitive....
A simple, accurate, precise and sensitive reverse phase high performance liquid chromatographic method was developed for simultaneous estimation of candesartan cilexetil and pioglitazone hydrochloride in synthetic mixture. C18, 250 mm X 4.6 mm, 5 μm particle size in isocratic mode with mobile phase acetonitrile: methanol: water (70:10:20 v/v/v) and pH adjusted to 5.0±0.1 with ortho phosphoric acid was used. The flow rate was 1.0 ml/min and absorbance of individual component was measured at 269 nm. The retention times of candesartan cilexetil and pioglitazone hydrochloride were found to be 8.11 and 4.23 min, respectively. Linearity for candesartan cilexetil and pioglitazone hydrochloride was in the range of 10-250 and 20-500 μg/ml with correlation coefficient values 0.9996 and 0.9997 the percentage recovery obtained was 99.50-99.73 % and 99.54-99.98 %, respectively....
The manuscript describes validated RP-HPLC method for simultaneous estimation of domperidone, tramadol hydrochloride and dicyclomine in tablet dosage form. The separation was achieved by C18 column (250×4.6 mm, 5 μm Particle Size) with mobile phase of 0.02 M KH2PO4, pH 6.5 Adjusted with NaOH (65:35%v/v) at 215 nm. Retention time of domperidone, tramadol hydrochloride and dicylomine was found to be 2.187 min, 2.827 min and 9.200 min, respectively. The method has been validated for linearity, accuracy and precision. Linearity was found in the range of 5-30 μg/ml, 25-150 μg/ml and 5-30 μg/ml for domperidone, tramadol hydrochloride and dicylomine respectively. The recoveries for domperidone, tramadol hydrochloride and dicylomine were found to be of 100.01±0.04%, 101.05±0.33% and 99.00±0.02% respectively in tablet. Developed method was found to be new, accurate, precise and rapid for simultaneous estimation of domperidone, tramadol hydrochloride and dicylomine in tablet dosage form....
A simple, accurate, reproducible, precise and economic reverse phase high performance liquid chromatographic method was developed for simultaneous estimation of clopidogrel bisulphate and irbesartan in synthetic mixture. Column used were phenomenex C18, 250 mm x 4.6 mm, 5 μm particle size in isocratic elution mode with mobile phase acetonitrile:0.2 M potassium dihydrogen orthophosphate (68:32 v/v) and pH adjusted to 4.0 with ortho phosphoric acid was used. The flow rate was 1.0 ml/min and absorbance of component was measured at 220 nm. The retention times of clopidogrel bisulphate and irbesartan were found to be 8.94 and 4.15 min, respectively. Linearity for both drugs clopidogrel bisulphate and irbesartan was in the range of 10-250 μg/ml with correlation coefficient values 0.9998 and 0.9997, the percentage recovery obtained was 99.26 and 99.56 %, respectively....
Two new simple, sensitive, rapid, accurate and reproducible methods (spectrophotometric and ion pair chromatography) have been developed for simultaneous estimation of verapamil (VER) from its pure and tablet dosage form. The first method involves multiwavelength spectrophotometric method (Method I) in which interference of HCTZ at 245 nm (wavelength for estimation of VAL) was removed by recording absorbance difference at 245 nm and 301 nm whereas HCTZ was estimated directly from its absorbance at 316 nm at which VAL shows no absorbance. Linearity of the response was demonstrated by VER in the concentration range of 10-60 g/ml with a square correlation coefficient (r2) of 0.9992. The second method utilizes ion pair chromatography (Method 2) on a HIQ sil ODS column (250 mm x 4.6 mm i.d.) using a mobile phase consisting methanol:water (70:30 v/v) pH adjusted to 7.4 with orthophosphoric acid and addition of 1% 1-hexanesulfonic acid monohydrate sodium salt as an ion pair reagent with UV detection at 220 nm over concentration range for VER is 10-90 µg/ml. Atenolol was used as the internal standard. The suggested procedures were checked using laboratory prepared mixtures and were applied successfully for the analysis of their tablet dosage form. The results of analysis were statistically analysed. Both the methods were validated as per ICH Q2B guidelines....
In this study a latest IR spectroscopic procedure was narrated for quantitative determination of amikacin sulphate from solid dosage form. For IR spectroscopic method KBr disc technique, base line method has been used. The specific absorption bands at 3253 cm-1 were chosen as OH stretching mainly for hydroxyl group respectively. In this method Beer’s law was followed in the concentration range 0.8 to 2.0% w/w in KBr disc. The regression equation was found to be y = 0.122 x-0.1233 with correlation coefficient 0.9973 and the assay was found to be 97.9% with RSD of 1.153%....
A simple accurate and precise Q-absorbance ratio spectrophotometric method has been developed for estimation of cefepime hydrochloride and sulbactam sodium in injection dosage form. The iso-absorptive point was found to be 240 nm. The beer-lambert law followed in concentration range 4-32 μg/ml at 240 nm for cefepime hydrochloride and in 2-16 μg/ml at 263 nm sulbactam sodium respectively. The method was validated statistically as per ICH guidelines. The method showed good reproducibility and recovery with % RSD less than 2....
The entire text of manuscript is enlightened about quality circle which encompasses a series of step improvements in a process that might arise from the troubleshooting efforts of negligence, inadequate attention, laxity, lack of discipline in pharmaceutical industries which leads to affect the reputation of industry close scrutiny by federal regulatory bodies. The expertise encompassed about quality circle traverses as unit operations or discrete activities routinely found within any manufacturing process in case of pharmaceutical manufacturing this would involve the quality process which is the need of pharma world. The proposed approach links core elements of risk management, assurance structures and governance with the foundation elements of organizational culture, change management and data and knowledge management. It identifies the main risk influences and how pharmaceutical organizations can mitigate the risks by creating a systematic approach and a culture conducive to compliance. The compliance approach will help pharma companies contain risk and improve profitability through the optimal use of resources, knowledge management and best practices....
A simple, accurate and precise spectroscopic method was developed for simultaneous estimation of saxagliptin hydrochloride and glibenclamide in synthetic mixture using first order derivative zero-crossing method. Saxagliptin hydrochloride showed zero crossing point at 315.00 nm while glibenclamide showed zero crossing point at 229.40 nm. The dA/dλ was measured at 229.40 nm for saxagliptin hydrochloride and 315.00 nm for glibenclamide and calibration curves were plotted as dA/dλ versus concentration, respectively. The method was found to be linear (r2>0.9995) in the range of 5-25 μg/ml for saxagliptin hydrochloride at 229.40 nm. The linear correlation was obtained (r2>0.9994) in the range of 5-25 μg/ml for glibenclamide at 315.00 nm. The limit of determination was 0.243μg/ml and 0.317μg/ml for saxagliptin hydrochloride and glibenclamide, respectively. The limit of quantification was 0.738 μg/ml and 0.960 μg/ml for saxagliptin hydrochloride and glibenclamide respectively. The accuracy of these method were evaluated by recovery studies and good recovery result were obtained greater than 99% shows first order derivation zero crossing. The method was successfully applied for simultaneous determination of saxagliptin hydrochloride and glibenclamide in binary mixture....
A simple, accurate and precise spectroscopic method was developed for simultaneous estimation of saxagliptin hydrochloride and glibenclamide in synthetic mixture using simultaneous equation method. The absorbance was measured at 210.00 nm for saxagliptin hydrochloride and 229.00 nm for glibenclamide and calibration curves were plotted as absorbance versus concentration, respectively. The method was found to be linear (r2>0.9995) in the range of 5-25 μg/ml for saxagliptin hydrochloride at 210.00 nm. The linear correlation was obtained (r2>0.9996) in the range of 5-25 μg/ml for glibenclamide at 229.00 nm. The limit of determination (LOD) was 0.307 μg/ml and 0.149 μg/ml for saxagliptin hydrochloride and glibenclamide respectively. The limit of quantification (LOQ) was 0.931 μg/ml and 0.452 μg/ml for saxagliptin hydrochloride and glibenclamide respectively. The accuracy of these method were evaluated by recovery studies and good recovery result were obtained greater than 99%.The method was successfully applied for simultaneous determination of saxagliptin hydrochloride and glibenclamide in binary mixture....
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